CN107601898B - Preparation method of Jun porcelain blue glaze - Google Patents
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Abstract
The invention provides a preparation method of Jun porcelain blue glaze, which consists of the following glaze materials in parts by weight: 20-25 parts of melilite, 12-18 parts of white feldspar, 10-15 parts of quartz stone, 10-15 parts of calcite, 10-12 parts of fluorite, 5-7 parts of plant ash, 4-6 parts of Ru bluestone, 3-5 parts of cobalt oxide, 3-5 parts of zirconium oxide, 2-4 parts of zinc oxide, 2-4 parts of aluminum oxide, 2-3 parts of tin oxide and 8-10 parts of fusion cake are processed to obtain glaze slurry, and then the glaze slurry, the auxiliary material and the protective agent are coated on a biscuit through a certain process to obtain a product.
Description
Technical Field
The invention relates to the technical field of Jun porcelain processing, in particular to a preparation method of Jun porcelain blue glaze.
Background
Jun porcelain is honored as the first of five famous porcelain in China, and is quite honored with gold valuable jun valueless and rather than with Jun porcelain. Jun porcelain is known as unique furnace transmutation art, however, the yield of the Jun porcelain is low, only 30% of the yield is achieved, and the superior Jun porcelain is rare. The main reason is that the jun porcelain is influenced by a plurality of factors in the firing process, and each link can directly cause the production failure of the jun porcelain, wherein the temperature change, the heating rate, the glazing method and the like in the kiln particularly have important influences on the jun porcelain production process.
The Jun porcelain kiln transformation means that glaze on the Jun porcelain can also change other colors besides natural glaze in the firing process, the Jun porcelain is precious in the unique kiln transformation glaze color, the glaze color is naturally formed in the firing process, the glaze generates gorgeous color changes when melted at high temperature, the painting is not artificially depicted, the glaze color of each Jun porcelain is unique, and therefore the Jun porcelain kiln transformation method has the 'Jun porcelain no-double' method, the glaze color changes generated by different firing processes are different, and the gorgeous Jun porcelain can be produced by adopting different firing processes.
Disclosure of Invention
The invention aims to provide a preparation method of Jun porcelain blue glaze, which is glittering and translucent in color and solves the problem that the color of the produced Jun porcelain is monotonous and uncontrollable.
The technical scheme adopted by the invention for solving the technical problems is as follows: a preparation method of Jun porcelain blue glaze comprises the following specific steps:
the method comprises the following steps: taking 20-25 parts of melilite, 12-18 parts of white feldspar, 10-15 parts of quartz stone, 10-15 parts of calcite and 10-12 parts of fluorite, putting the materials into a ball mill for grinding, and screening to obtain mixed powder a with the granularity of 10-40 mu m for later use;
step two: taking 5-7 parts of plant ash, 4-6 parts of Ru bluestone, 3-5 parts of cobalt oxide, 3-5 parts of zirconium oxide, 2-4 parts of zinc oxide, 2-4 parts of aluminum oxide and 2-3 parts of tin oxide, carrying out ball milling, and grinding and screening mixed powder b with the particle size of 120-160 mu m for later use;
step three: ball-milling 8-10 parts of fusion cake, and screening to obtain powder c with the particle size of 100-150 mu m for later use;
step four: adding the mixed powder a and the mixed powder b obtained in the first step and the second step into a muffle furnace for pre-sintering, preserving heat for 0.5-2 h at 200 ℃, then opening the muffle furnace for natural cooling at room temperature to obtain pre-sintered powder for later use;
step five: ball-milling the pre-sintering powder obtained in the fourth step, and grinding and screening the pre-sintering powder d with the granularity of 100-150 mu m for later use;
step six: standby in the third step and the fifth step: adding the powder c and the pre-sintering powder d into a mixer, then adding a proper amount of water, and carrying out fine grinding for 2-4 h to obtain glaze slurry;
step seven: glazing the plain blank by using the glaze slip obtained in the sixth step for the first time, and then drying at 120-150 ℃ to obtain a first semi-finished product;
step eight: and C, performing primary sintering on the semi-finished product in the step seven, wherein the primary sintering process specifically comprises the following steps:
⑴, a first oxidation period, namely putting the semi-finished product in the step seven into a kiln, heating the semi-finished product from room temperature to 380-410 ℃ at a heating rate of 1-2 ℃/min in an air atmosphere, then closing a skylight at the top of the kiln, gradually heating the semi-finished product in an oxidation atmosphere at a heating rate of 2-4 ℃/min, and heating the temperature in the kiln to 1050-1070 ℃;
⑵, in the reduction period, the temperature is increased to 1140-1160 ℃ at the temperature rising rate of 4-7 ℃/min in the reduction atmosphere;
⑶, in a neutral period, raising the temperature to 1260-1270 ℃ at a temperature raising rate of 0.5-1.5 ℃/min under a weak reducing atmosphere;
⑷, in the second oxidation period, raising the temperature to 1280-1290 ℃ at the rate of 0.5-1 ℃/min, preserving the heat for 1-3 h, immediately stopping the fire, and then opening the kiln door for natural cooling to obtain a first fired product;
step nine, uniformly coating a layer of auxiliary materials on the surface of the first firing product obtained in the step ⑷ in the step eight, and then putting the first firing product into a kiln for secondary firing to obtain a second firing product;
step ten: glazing the second fired finished product obtained in the ninth step by using the glaze slip obtained in the sixth step, drying at 120-150 ℃ to obtain a second semi-finished product, and then placing into a kiln for firing for the third time to obtain a third fired finished product;
step eleven: uniformly coating a layer of protective agent on the third fired product obtained in the sixth step, wherein the protective agent is a frit, and the pretreatment method of the protective agent comprises the following steps: putting the frit with the particle size of 80-120 mu m into a ball mill for grinding for 1-4 h, adding a proper amount of water for wet grinding for 1-3 h; and (3) putting the third firing product coated with the protective agent into a kiln, firing for the fourth time at a heating rate of 3-5 ℃/min, preserving heat at 900-950 ℃ for 2-3 h, and directly opening the kiln for cooling to obtain the product.
Further, the ratio of the water added in the sixth step to the total mass of the mixed powder a, the mixed powder b and the mixed powder c is 1: 1.1-1: 2.
Further, the temperature rising rate of the pre-sintering in the fourth step is 2-4 ℃/min.
Furthermore, the second firing process and the third firing process are the same as the first firing process.
Further, the mass ratio of the added auxiliary materials to the sum of the mixed powder a, the mixed powder b and the mixed powder c is 0.01: 1-0.05: 1.
Further, the auxiliary material is prepared from the following raw materials in parts by weight: 50-60 parts of fusion cake and 40-50 parts of calcium carbonate.
Further, the preparation method of the auxiliary material comprises the following steps of taking 50-60 parts of fusion cakes and 40-50 parts of calcium carbonate, carrying out ball milling, placing the fusion cakes and the calcium carbonate into a muffle furnace for sintering, placing the fusion cakes and the calcium carbonate to room temperature, adding a proper amount of water for wet milling, and carrying out wet milling for 2-4 hours for later use.
Further, the mass ratio of the protective agent to the sum of the mixed powder a, the mixed powder b and the powder c is 0.05: 1-0.1: 1.
Furthermore, the particle sizes of the melilite, the albite, the quartz stone, the calcite and the fluorite are 10-40 mu m.
Furthermore, the particle size of the frit, plant ash, Ru kyanite, cobalt oxide, zirconium oxide, zinc oxide, aluminum oxide and tin oxide is 20-50 μm.
The beneficial effects of the invention are mainly expressed as follows: the invention provides a novel Jun porcelain glaze formula, and the production and processing processes of the glaze are described in detail, the glaze is ground in batches, the particle sizes of the components of the glaze are refined, and the mixed powder a and the mixed powder b are added into a muffle furnace for pre-burning, so that residual gas in gaps between the mixed powder a and the mixed powder b can be discharged, and the prepared Jun porcelain has the advantages of reduced cracks, very transparent surface, good fluidity, uniform color, increased stereoscopic impression and difficult bubbling, and the surface of the Jun porcelain has strong mechanical force; drying the biscuit body after the first glazing at 120-150 ℃, primarily drying the biscuit body glaze at a low temperature, primarily discharging water in the surface layer of the glaze, and avoiding cracks on the surface layer of the glaze due to too high drying rate under a high temperature condition; the first firing is carried out, in the first oxidation period, the temperature is raised to 380-410 ℃ from room temperature in the air atmosphere, the temperature raising rate is 1-2 ℃/min, and a smaller temperature raising speed is adopted in the temperature interval, because the temperature period is used for removing moisture in a sagger, a product and a kiln, and if a higher temperature raising rate is adopted, the moisture in the product can cause gas expansion due to rapid volatilization to cause product explosion; obtaining a first fired product through a reduction period, a neutral period and a second oxidation period; uniformly coating a layer of auxiliary material on the surface of the first fired product, wherein the auxiliary material consists of frit and calcium carbonate, the frit is formed by melting and quenching glass at high temperature, ball-milling the frit and the calcium carbonate, then putting the frit and the calcium carbonate into a muffle furnace for sintering, combining the frit and the calcium carbonate in the sintering process, cooling, adding a proper amount of water, ball-milling the frit and the calcium carbonate again, uniformly coating the auxiliary material on the surface of the first fired product, then putting the first fired product into a kiln for secondary firing, decomposing the calcium carbonate in the auxiliary material into calcium oxide and carbon dioxide at high temperature in the secondary firing process, and uniformly forming a plurality of tiny adsorption holes on the surface of the second fired product after the secondary firing; the glaze is glazed for the second time on the second fired product, so that the glaze can be better adsorbed on the surface of the second fired product through the adsorption holes; and finally, uniformly coating a layer of protective agent which is frit on the third sintered product, uniformly coating the frit on the surface of the third sintered product after wet grinding, and then performing fourth sintering, so that the frit on the surface of the third sintered product forms a protective vitreous substance on the surface of the Jun porcelain through high temperature in the fourth sintering process to prevent the surface of the Jun porcelain from being scratched carelessly.
Detailed Description
The present invention is described in detail with reference to the following examples, which are provided for the purpose of explaining the technical solutions of the present invention and describing the detailed embodiments and the specific operation procedures, but the scope of the present invention is not limited to the following examples.
Example one
A preparation method of Jun porcelain blue glaze comprises the following specific steps:
the method comprises the following steps: taking 20 parts of melilite, 12 parts of white feldspar, 10 parts of quartz stone, 10 parts of calcite and 10 parts of fluorite, putting the materials into a ball mill for grinding, and screening to obtain mixed powder a with the granularity of 10-40 mu m for later use;
step two: taking 5 parts of plant ash, 4 parts of Ru kyanite, 3 parts of cobalt oxide, 3 parts of zirconium oxide, 2 parts of zinc oxide, 2 parts of aluminum oxide and 2 parts of tin oxide, carrying out ball milling, and grinding and screening mixed powder b with the granularity of 120-160 mu m for later use;
step three: ball-milling 8 parts of fusion cake, and screening to obtain powder c with the particle size of 100-150 mu m for later use;
step four: adding the mixed powder a and the mixed powder b obtained in the first step and the second step into a muffle furnace for pre-sintering, preserving the heat for 0.5-2 h at 200 ℃, then opening the muffle furnace for natural cooling at room temperature to obtain pre-sintered powder for later use;
step five: ball-milling the pre-sintering powder obtained in the fourth step, and grinding and screening the pre-sintering powder d with the granularity of 100-150 mu m for later use;
step six: standby in the third step and the fifth step: adding the powder c and the pre-sintering powder d into a mixer, then adding a proper amount of water, and carrying out fine grinding for 2 hours to obtain glaze slurry;
step seven: glazing the plain blank by the glaze slip obtained in the sixth step for the first time, and then drying at 120 ℃ to obtain a first semi-finished product;
step eight: and C, performing primary sintering on the semi-finished product in the step seven, wherein the primary sintering process specifically comprises the following steps:
⑴, a first oxidation period, namely putting the semi-finished product in the step seven into a kiln, heating the semi-finished product from room temperature to 380 ℃ in an air atmosphere at a heating rate of 1 ℃/min, then closing a skylight at the top of the kiln, gradually heating the semi-finished product in an oxidation atmosphere at a heating rate of 2 ℃/min, and heating the temperature in the kiln to 1050-1070 ℃;
⑵, a reduction period, namely, in a reduction atmosphere, raising the temperature to 1140-1160 ℃ at a temperature raising rate of 4 ℃/min;
⑶, in a neutral period, raising the temperature to 1260-1270 ℃ at a temperature raising rate of 0.5 ℃/min in a weak reducing atmosphere;
⑷, in the second oxidation period, raising the temperature to 1280-1290 ℃ at the rate of 0.5 ℃/min, keeping the temperature for 1h, immediately stopping heating, and then opening a kiln door for natural cooling to obtain a first fired product;
step nine, uniformly coating a layer of auxiliary materials on the surface of the first firing product obtained in the step ⑷ in the step eight, and then putting the first firing product into a kiln for secondary firing to obtain a second firing product;
step ten: glazing the second fired finished product obtained in the ninth step by using the glaze slip obtained in the sixth step, drying at 120-150 ℃ to obtain a second semi-finished product, and then placing into a kiln for firing for the third time to obtain a third fired finished product;
step eleven: uniformly coating a layer of protective agent on the third fired product obtained in the sixth step, wherein the protective agent is a frit, and the pretreatment method of the protective agent comprises the following steps: putting the frit with the particle size of 80-120 mu m into a ball mill for grinding for 1h, adding a proper amount of water for wet grinding for 1 h; and (3) putting the third firing product coated with the protective agent into a kiln, firing for the fourth time at the heating rate of 3 ℃/min, preserving heat at 930 ℃ for 2h, and directly opening the kiln for cooling to obtain the product.
Further, the ratio of the water added in the sixth step to the sum of the mixed powder a, the mixed powder b and the mixed powder c is 1: 1.1.
Further, the temperature rising rate of the pre-sintering in the fourth step is 2 ℃/min.
Furthermore, the second firing process and the third firing process are the same as the first firing process.
Further, the mass ratio of the added auxiliary materials to the sum of the mass of the mixed powder a, the mass of the mixed powder b and the mass of the mixed powder c is 0.01: 1.
Further, the auxiliary material is prepared from the following raw materials in parts by weight: 50 parts of clinker and 40 parts of calcium carbonate.
Further, the preparation method of the auxiliary material comprises the following steps of taking 50 parts of fusion cake and 40 parts of calcium carbonate, carrying out ball milling, placing into a muffle furnace for sintering, placing to room temperature, adding a proper amount of water for wet milling, and carrying out wet milling for 2 hours for later use.
Further, the mass ratio of the protective agent to the sum of the mass of the mixed powder a, the mass of the mixed powder b and the mass of the mixed powder c is 0.05: 1.
Furthermore, the particle sizes of the melilite, the albite, the quartz stone, the calcite and the fluorite are 10-40 mu m.
Furthermore, the particle size of the frit, plant ash, Ru kyanite, cobalt oxide, zirconium oxide, zinc oxide, aluminum oxide and tin oxide is 20-50 μm.
Example two
A preparation method of Jun porcelain blue glaze comprises the following specific steps:
the method comprises the following steps: taking 25 parts of melilite, 18 parts of white feldspar, 15 parts of quartz stone, 15 parts of calcite and 12 parts of fluorite, putting the materials into a ball mill for grinding, and screening to obtain mixed powder a with the granularity of 10-40 mu m for later use;
step two: taking 7 parts of plant ash, 6 parts of Ru kyanite, 5 parts of cobalt oxide, 5 parts of zirconium oxide, 4 parts of zinc oxide, 4 parts of aluminum oxide and 3 parts of tin oxide, carrying out ball milling, and grinding and screening mixed powder b with the granularity of 120-160 mu m for later use;
step three: ball-milling 10 parts of fusion cake, and screening to obtain powder c with the particle size of 100-150 mu m for later use;
step four: adding the mixed powder a and the mixed powder b obtained in the first step and the second step into a muffle furnace for pre-sintering, preserving heat for 2 hours at 200 ℃, then opening the muffle furnace for natural cooling at room temperature to obtain pre-sintered powder for later use;
step five: ball-milling the pre-sintering powder obtained in the fourth step, and grinding and screening the pre-sintering powder d with the granularity of 100-150 mu m for later use;
step six: standby in the third step and the fifth step: adding the powder c and the pre-sintering powder d into a mixer, then adding a proper amount of water, and carrying out fine grinding for 4 hours to obtain glaze slurry;
step seven: glazing the plain blank by using the glaze slip obtained in the sixth step for the first time, and then drying at 120-150 ℃ to obtain a first semi-finished product;
step eight: and C, performing primary sintering on the semi-finished product in the step seven, wherein the primary sintering process specifically comprises the following steps:
⑴, a first oxidation period, namely putting the semi-finished product in the step seven into a kiln, heating the semi-finished product from room temperature to 410 ℃ at a heating rate of 2 ℃/min in an air atmosphere, then closing a skylight at the top of the kiln, gradually heating the semi-finished product in an oxidation atmosphere at a heating rate of 4 ℃/min, and heating the temperature in the kiln to 1050-1070 ℃;
⑵, a reduction period, namely, in a reduction atmosphere, raising the temperature to 1140-1160 ℃ at a temperature raising rate of 7 ℃/min;
⑶, in a neutral period, raising the temperature to 1260-1270 ℃ at a temperature raising rate of 1.5 ℃/min in a weak reducing atmosphere;
⑷, in the second oxidation period, raising the temperature to 1280-1290 ℃ at the heating rate of 1 ℃/min, keeping the temperature for 3 hours, immediately stopping heating, and then opening a kiln door for natural cooling to obtain a first fired product;
step nine, uniformly coating a layer of auxiliary materials on the surface of the first firing product obtained in the step ⑷ in the step eight, and then putting the first firing product into a kiln for secondary firing to obtain a second firing product;
step ten: glazing the second fired finished product obtained in the ninth step by using the glaze slip obtained in the sixth step, drying at 120-150 ℃ to obtain a second semi-finished product, and then placing into a kiln for firing for the third time to obtain a third fired finished product;
step eleven: uniformly coating a layer of protective agent on the third fired product obtained in the sixth step, wherein the protective agent is a frit, and the pretreatment method of the protective agent comprises the following steps: putting the frit with the particle size of 80-120 mu m into a ball mill for grinding for 4h, adding a proper amount of water for wet grinding, and performing wet grinding for 3 h; and (3) putting the third firing product coated with the protective agent into a kiln, firing for the fourth time at the heating rate of 5 ℃/min, preserving heat at 900-950 ℃ for 3h, and directly opening the kiln for cooling to obtain the product.
Further, the ratio of the water added in the sixth step to the sum of the mixed powder a, the mixed powder b and the mixed powder c is 1: 2.
Further, the temperature rising rate of the pre-sintering in the fourth step is 4 ℃/min.
Furthermore, the second firing process and the third firing process are the same as the first firing process.
Further, the mass ratio of the added auxiliary materials to the sum of the mass of the mixed powder a, the mass of the mixed powder b and the mass of the mixed powder c is 0.05: 1.
Further, the auxiliary material is prepared from the following raw materials in parts by weight: 60 parts of clinker and 50 parts of calcium carbonate.
Further, the preparation method of the auxiliary material comprises the following steps of taking 60 parts of fusion cake and 50 parts of calcium carbonate to perform ball milling, putting the fusion cake and the calcium carbonate into a muffle furnace to perform sintering, standing the mixture to room temperature, adding a proper amount of water to perform wet milling, and performing wet milling for 4 hours for later use.
Further, the mass ratio of the protective agent to the sum of the mass of the mixed powder a, the mass of the mixed powder b and the mass of the mixed powder c is 0.1: 1.
Furthermore, the particle sizes of the melilite, the albite, the quartz stone, the calcite and the fluorite are 10-40 mu m.
Furthermore, the particle size of the frit, plant ash, Ru kyanite, cobalt oxide, zirconium oxide, zinc oxide, aluminum oxide and tin oxide is 20-50 μm.
EXAMPLE III
A preparation method of Jun porcelain blue glaze comprises the following specific steps:
the method comprises the following steps: taking 23 parts of melilite, 16 parts of white feldspar, 13 parts of quartz stone, 13 parts of calcite and 11 parts of fluorite, putting the materials into a ball mill for grinding, and screening to obtain mixed powder a with the granularity of 10-40 mu m for later use;
step two: taking 6 parts of plant ash, 5 parts of Ru kyanite, 4 parts of cobalt oxide, 4 parts of zirconium oxide, 3 parts of zinc oxide, 3 parts of aluminum oxide and 2.5 parts of tin oxide, carrying out ball milling, and grinding and screening mixed powder b with the granularity of 120-160 mu m for later use;
step three: ball-milling 9 parts of fusion cake, and screening to obtain powder c with the particle size of 100-150 mu m for later use;
step four: adding the mixed powder a and the mixed powder b obtained in the first step and the second step into a muffle furnace for pre-sintering, preserving heat for 1h at 200 ℃, then opening the muffle furnace, and naturally cooling at room temperature to obtain pre-sintered powder for later use;
step five: ball-milling the pre-sintering powder obtained in the fourth step, and grinding and screening the pre-sintering powder d with the granularity of 100-150 mu m for later use;
step six: standby in the third step and the fifth step: adding the powder c and the pre-sintering powder d into a mixer, then adding a proper amount of water, and carrying out fine grinding for 3 hours to obtain glaze slurry;
step seven: glazing the plain blank by using the glaze slip obtained in the sixth step for the first time, and then drying at 120-150 ℃ to obtain a first semi-finished product;
step eight: and C, performing primary sintering on the semi-finished product in the step seven, wherein the primary sintering process specifically comprises the following steps:
⑴, a first oxidation period, namely putting the semi-finished product in the step seven into a kiln, heating the semi-finished product from room temperature to 390 ℃ in an air atmosphere at a heating rate of 1.5 ℃/min, then closing a skylight at the top of the kiln, gradually heating the semi-finished product in an oxidation atmosphere at a heating rate of 3 ℃/min, and heating the temperature in the kiln to 1050-1070 ℃;
⑵, in the reduction period, the temperature is increased to 1140-1160 ℃ at the temperature rising rate of 5.5 ℃/min in the reduction atmosphere;
⑶, in a neutral period, raising the temperature to 1260-1270 ℃ at a temperature raising rate of 1 ℃/min under a weak reducing atmosphere;
⑷, in the second oxidation period, raising the temperature to 1280-1290 ℃ at the rate of 0.75 ℃/min, preserving the heat for 2 hours, immediately stopping the fire, and then opening the kiln door for natural cooling to obtain a first fired product;
step nine, uniformly coating a layer of auxiliary materials on the surface of the first firing product obtained in the step ⑷ in the step eight, and then putting the first firing product into a kiln for secondary firing to obtain a second firing product;
step ten: glazing the second fired finished product obtained in the ninth step by using the glaze slip obtained in the sixth step, drying at 120-150 ℃ to obtain a second semi-finished product, and then placing into a kiln for firing for the third time to obtain a third fired finished product;
step eleven: uniformly coating a layer of protective agent on the third fired product obtained in the sixth step, wherein the protective agent is a frit, and the pretreatment method of the protective agent comprises the following steps: putting the frit with the particle size of 80-120 mu m into a ball mill for grinding for 2.5h, adding a proper amount of water for wet grinding for 2 h; and (3) putting the third firing product coated with the protective agent into a kiln, firing for the fourth time at the heating rate of 4 ℃/min, preserving heat for 2.5 hours at 900-950 ℃, and directly opening the kiln to cool to obtain the product.
Further, the ratio of the water added in the sixth step to the sum of the mixed powder a, the mixed powder b and the mixed powder c is 1: 1.5.
Further, the temperature rising rate of the pre-sintering in the fourth step is 3 ℃/min.
Furthermore, the second firing process and the third firing process are the same as the first firing process.
Further, the mass ratio of the added auxiliary materials to the total mass of the mixed powder a, the mixed powder b and the mixed powder c is 0.03: 1.
Further, the auxiliary material is prepared from the following raw materials in parts by weight: 55 parts of frit and 45 parts of calcium carbonate.
Further, the preparation method of the auxiliary material comprises the following steps of taking 55 parts of fusion cake and 45 parts of calcium carbonate, carrying out ball milling, placing into a muffle furnace for sintering, placing to room temperature, adding a proper amount of water for wet milling, and carrying out wet milling for 3 hours for later use.
Further, the mass ratio of the protective agent to the sum of the mass of the mixed powder a, the mixed powder b and the powder c is 0.075: 1.
Furthermore, the particle sizes of the melilite, the albite, the quartz stone, the calcite and the fluorite are 10-40 mu m.
Furthermore, the particle size of the frit, plant ash, Ru kyanite, cobalt oxide, zirconium oxide, zinc oxide, aluminum oxide and tin oxide is 20-50 μm.
The feldspar belongs to silicate mineral salts, contains potassium element, sodium element, calcium element and the like in the internal content, is divided into yellow, white, red and the like, is a main component of the glaze, and mainly plays an important role in forming the glaze. Numerous mineral deposits are distributed in Yuzhou;
the calcite mainly reduces the melting temperature of the glaze, increases the glossiness and transparency of the glaze color, prevents and controls cracking and accumulation of the glaze, and cannot be used in an excessive amount, otherwise, the glaze can be devitrified and devitrified, the temperature is narrowed, the change is too little, and the glaze smokes;
fluorite is a mineral, an isometric crystal system, the main component of the fluorite is calcium fluoride, the melting temperature of glaze can be reduced, the fluidity of the glaze is increased, and meanwhile, the fluorite has an opacifying effect, can improve the glossiness of Jun glaze and improves the suspension property of glaze slurry;
quartz is commonly used in Jun porcelain glaze; the plant ash is pine ash;
zinc oxide is a commonly used chemical additive, and is widely applied to the manufacture of products such as plastics, silicate products, synthetic rubber, lubricating oil, paint, coating, ointment, adhesive, food, batteries, flame retardant and the like. The zinc oxide has larger energy band gap and exciton binding energy, high transparency and excellent normal-temperature luminous performance;
the frit has insolubility and stability, is prepared for standby after being processed and ground, can be used as a strong solvent for glaze, and can also be used independently. The frit is formed by melting and quenching glass at high temperature; grinding, applying on Jun porcelain, and firing to obtain a thin layer of vitreous material; zirconium oxide is used as a main coloring agent of the azure jun porcelain glaze,
the tin oxide is white, light yellow or light gray tetragonal, hexagonal or orthorhombic powder. Melting point 1630 ℃;
the zirconium dioxide is added in the invention, so that the aluminum oxide grains can be refined, and the compactness of the glaze in the sintering process is increased; copper oxide is a common colorant in Jun porcelain glaze;
the main component of the Ru bluestone is silicon dioxide, and the Ru bluestone is a stone for preparing Jun porcelain glaze and is described in detail in the book of Chinese Jun furnace research of Henan people press;
according to the invention, natural raw materials and chemical raw materials are matched and interacted, so that under the action of high-temperature melting, a unique glaze color is produced, and the method has good social and economic benefits;
the invention provides a preparation method of porcelain blue glaze, which comprises the steps of grinding glaze in batches, refining the particle sizes of components of the glaze, adding mixed powder a and mixed powder b into a muffle furnace for pre-burning, and discharging residual gas in gaps between the mixed powder a and the mixed powder b, so that cracks of a glaze surface on the prepared Jun porcelain are reduced, the surface is very transparent, the fluidity is good, the color is uniform, the stereoscopic impression is increased, the porcelain blue glaze is not easy to bubble, and the surface of the Jun porcelain has stronger mechanical force; drying the biscuit body after the first glazing at 120-150 ℃, primarily drying the biscuit body glaze at a low temperature, primarily discharging water in the surface layer of the glaze, and avoiding cracks on the surface layer of the glaze due to too high drying rate under a high temperature condition; the first firing is carried out, in the first oxidation period, the temperature is raised to 380-410 ℃ from room temperature in the air atmosphere, the temperature raising rate is 1-2 ℃/min, and a smaller temperature raising speed is adopted in the temperature interval, because the temperature period is used for removing moisture in a sagger, a product and a kiln, and if a higher temperature raising rate is adopted, the moisture in the product can cause gas expansion due to rapid volatilization to cause product explosion; obtaining a first fired product through a reduction period, a neutral period and a second oxidation period; uniformly coating a layer of auxiliary material on the surface of the first fired product, wherein the auxiliary material consists of frit and calcium carbonate, the frit is formed by melting and quenching glass at high temperature, ball-milling the frit and the calcium carbonate, then putting the frit and the calcium carbonate into a muffle furnace for sintering, combining the frit and the calcium carbonate in the sintering process, cooling, adding a proper amount of water, ball-milling the frit and the calcium carbonate again, uniformly coating the auxiliary material on the surface of the first fired product, then putting the first fired product into a kiln for secondary firing, decomposing the calcium carbonate in the auxiliary material into calcium oxide and carbon dioxide at high temperature in the secondary firing process, and uniformly forming a plurality of tiny adsorption holes on the surface of the second fired product after the secondary firing; the glaze is glazed for the second time on the second fired product, so that the glaze can be better adsorbed on the surface of the second fired product through the adsorption holes; and finally, uniformly coating a layer of protective agent which is frit on the third sintered product, uniformly coating the frit on the surface of the third sintered product after wet grinding, and then performing fourth sintering, so that the frit on the surface of the third sintered product forms a protective vitreous substance on the surface of the Jun porcelain through high temperature in the fourth sintering process to prevent the surface of the Jun porcelain from being scratched carelessly.
It is further noted that relational terms such as i, ii, iii, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
Claims (10)
1. A preparation method of Jun porcelain blue glaze is characterized by comprising the following steps:
the method comprises the following steps: taking 20-25 parts of melilite, 12-18 parts of white feldspar, 10-15 parts of quartz stone, 10-15 parts of calcite and 10-12 parts of fluorite, putting the materials into a ball mill for grinding, and screening to obtain mixed powder a with the granularity of 10-40 mu m for later use;
step two: taking 5-7 parts of plant ash, 4-6 parts of Ru bluestone, 3-5 parts of cobalt oxide, 3-5 parts of zirconium oxide, 2-4 parts of zinc oxide, 2-4 parts of aluminum oxide and 2-3 parts of tin oxide, carrying out ball milling, and grinding and screening mixed powder b with the particle size of 120-160 mu m for later use;
step three: ball-milling 8-10 parts of fusion cake, and screening to obtain powder c with the particle size of 100-150 mu m for later use;
step four: adding the mixed powder a and the mixed powder b obtained in the first step and the second step into a muffle furnace for pre-sintering, preserving heat for 0.5-2 h at 200 ℃, then opening the muffle furnace for natural cooling at room temperature to obtain pre-sintered powder for later use;
step five: ball-milling the pre-sintering powder obtained in the fourth step, and grinding and screening the pre-sintering powder d with the granularity of 100-150 mu m for later use;
step six: adding the powder c to be used and the pre-sintering powder d in the third step and the fifth step into a mixer, then adding a proper amount of water, and carrying out fine grinding for 2-4 h to obtain glaze slurry;
step seven: glazing the plain blank by using the glaze slip obtained in the sixth step for the first time, and then drying at 120-150 ℃ to obtain a first semi-finished product;
step eight: and C, performing primary sintering on the semi-finished product in the step seven, wherein the primary sintering process specifically comprises the following steps:
⑴, a first oxidation period, namely putting the semi-finished product in the step seven into a kiln, heating the semi-finished product to 400 ℃ from room temperature in an air atmosphere at a heating rate of 1-2 ℃/min, then closing a skylight at the top of the kiln, gradually heating the semi-finished product in an oxidation atmosphere at a heating rate of 2-4 ℃/min, and heating the temperature in the kiln to 1050-1070 ℃;
⑵, in the reduction period, the temperature is increased to 1140-1160 ℃ at the temperature rising rate of 4-7 ℃/min in the reduction atmosphere;
⑶, in a neutral period, raising the temperature to 1260-1270 ℃ at a temperature raising rate of 0.5-1.5 ℃/min under a weak reducing atmosphere;
⑷, in the second oxidation period, raising the temperature to 1280-1290 ℃ at the rate of 0.5-1 ℃/min, preserving the heat for 1-3 h, immediately stopping the fire, and then opening the kiln door for natural cooling to obtain a first fired product;
step nine, uniformly coating a layer of auxiliary materials on the surface of the first firing product obtained in the step ⑷ in the step eight, and then putting the first firing product into a kiln for secondary firing to obtain a second firing product;
step ten: glazing the second fired finished product obtained in the ninth step by using the glaze slip obtained in the sixth step, drying at 120-150 ℃ to obtain a second semi-finished product, and then placing into a kiln for firing for the third time to obtain a third fired finished product;
step eleven: uniformly coating a layer of protective agent on the third fired product obtained in the step ten, wherein the protective agent is a frit, and the pretreatment method of the protective agent comprises the following steps: putting the frit with the particle size of 80-120 mu m into a ball mill for grinding for 1-4 h, adding a proper amount of water for wet grinding for 1-3 h; and (3) putting the third firing product coated with the protective agent into a kiln, firing for the fourth time at a heating rate of 3-5 ℃/min, preserving heat at 900-950 ℃ for 2-3 h, and directly opening the kiln for cooling to obtain the product.
2. The preparation method of Jun porcelain blue glaze according to claim 1, characterized in that: and the mass ratio of the water to the total mass of the mixed powder a, the mixed powder b and the mixed powder c added in the sixth step is 1: 1.1-1: 2.
3. The preparation method of Jun porcelain blue glaze according to claim 1, characterized in that: and the temperature rising rate of the pre-sintering in the fourth step is 2-4 ℃/min.
4. The preparation method of Jun porcelain blue glaze according to claim 1, characterized in that: the second sintering process and the third sintering process are the same as the first sintering process.
5. The preparation method of Jun porcelain blue glaze according to claim 1, characterized in that: the mass ratio of the auxiliary materials to the sum of the mixed powder a, the mixed powder b and the mixed powder c is 0.01: 1-0.05: 1.
6. The preparation method of Jun porcelain blue glaze according to claim 1, characterized in that: the auxiliary material is prepared from the following raw materials in parts by weight: 50-60 parts of fusion cake and 40-50 parts of calcium carbonate.
7. The preparation method of Jun porcelain blue glaze according to claim 1, characterized in that: the preparation method of the auxiliary material comprises the following steps of taking 50-60 parts of fusion cakes and 40-50 parts of calcium carbonate to perform ball milling, placing the fusion cakes and the calcium carbonate into a muffle furnace to perform sintering, placing the fusion cakes and the calcium carbonate to room temperature, adding a proper amount of water to perform wet milling, and performing wet milling for 2-4 hours for later use.
8. The preparation method of Jun porcelain blue glaze according to claim 1, characterized in that: the mass ratio of the protective agent to the sum of the mixed powder a, the mixed powder b and the powder c is 0.05-0.1: 1.
9. The preparation method of Jun porcelain blue glaze according to claim 1, characterized in that: the particle sizes of the melilite, the albite, the quartz stone, the calcite and the fluorite are 10-40 mu m.
10. The preparation method of Jun porcelain blue glaze according to claim 1, characterized in that: the particle size of the frit, plant ash, Ru kyanite, cobalt oxide, zirconium oxide, zinc oxide, aluminum oxide and tin oxide is 20-50 mu m.
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| CN113896422B (en) * | 2021-11-18 | 2023-05-09 | 福建省德化县顺华达瓷业有限责任公司 | Kiln transition blue glaze, preparation method thereof and glaze firing method |
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